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EP0078435B1 - Clamping device for columns in chromatography - Google Patents

Clamping device for columns in chromatography Download PDF

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Publication number
EP0078435B1
EP0078435B1 EP82109585A EP82109585A EP0078435B1 EP 0078435 B1 EP0078435 B1 EP 0078435B1 EP 82109585 A EP82109585 A EP 82109585A EP 82109585 A EP82109585 A EP 82109585A EP 0078435 B1 EP0078435 B1 EP 0078435B1
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EP
European Patent Office
Prior art keywords
column
clamping
columns
sealing elements
sealing
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired
Application number
EP82109585A
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German (de)
French (fr)
Other versions
EP0078435A3 (en
EP0078435A2 (en
Inventor
Günther Sättler
Werner Gunkel
Manfred Witzgall
Reinhard Look
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Merck Patent GmbH
Original Assignee
Merck Patent GmbH
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
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Publication of EP0078435A2 publication Critical patent/EP0078435A2/en
Publication of EP0078435A3 publication Critical patent/EP0078435A3/en
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Publication of EP0078435B1 publication Critical patent/EP0078435B1/en
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/60—Construction of the column
    • G01N30/6047—Construction of the column with supporting means; Holders
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
    • G01N2030/8881—Modular construction, specially adapted therefor
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/60—Construction of the column
    • G01N30/6004—Construction of the column end pieces
    • G01N30/6021—Adjustable pistons

Definitions

  • the invention relates to a device for clamping and quickly changing columns for liquid chromatography, with a dead volume-free connection of the column and connecting pieces, which contain feeds and discharges for the eluent, by the interaction of sealing elements of the column and the connecting pieces.
  • a variant of this solution is that the column is designed as a cartridge sealed on both sides with a filter medium. This is clamped into a tube with reducing fittings on both sides and connecting fittings for the capillaries.
  • the advantage of this construction is that when the column has to be changed, only the cartridge containing the sorbent has to be replaced, whereas the complicated and expensive reducing screw connections can be used again and again.
  • the capillary line must be removed at least on one side before unscrewing the reducing screw.
  • a similar device is known from US-A 3,682,315.
  • connection connections which are essential for a good separation performance of the column are produced by manual screwing. There is always the risk that either a too tight tightening will not achieve a complete seal or that the sealing elements will be damaged by overtightening. A quick, safe column change, even by inexperienced personnel, is therefore not possible. An automated column change is hardly possible.
  • the object was therefore to find a clamping device which allows a quick, possibly also automated column change and which nevertheless ensures improved safety of the seal.
  • the invention therefore relates to a device for clamping and rapidly changing columns for liquid chromatography according to claim 1.
  • 1 denotes a carrier plate
  • 2 the column and 3 the lower tensioning and sealing element
  • 4 is a bearing
  • 5 the upper tensioning and sealing element
  • 6 a pressure element with the stamp 7.
  • a centering piece is designated by 8
  • g and 10 are capillaries for the solvent supply and discharge.
  • 11 is a sealing cone specially designed for the connection of a cartridge
  • 12 is the column filling.
  • 13 is a sealing ring with a pressed-in frit 14, which is fastened to the end of the cartridge with a glued-on or pressed-on cap 15.
  • 16 with a frit and 17 denotes a sealing ring, which are pressed into a reducing screw 18.
  • 19 is a clamping and sealing element specially adapted to columns with reducing screw connection and 20 the corresponding sealing cone.
  • 21 is a frit, 22 a ball bed and 23 a seal.
  • 24 is a further embodiment of a tensioning and sealing element.
  • 25 is a flexible membrane and 26 is a clamping cap. With 27 a pressure ring for holding the clamping cap 26 is designated, with 28 a stamp, with 29 a clamping element and with 30 a spring element.
  • 31 is a rotating magazine, 32 is a clamping and sealing element and 33 is a pneumatic cylinder.
  • the device according to the invention can be used in connection with all possible column constructions.
  • only the sealing part of the tensioning and sealing element (5, 19/20, 24, 27/28) must be matched to the column.
  • the principle according to the invention namely that the column is clamped between two clamping and sealing elements without screwing, remains unaffected. It can therefore both Columns according to FIG. 4 that are still predominantly used today are used as well as cartridge columns according to FIG. 3 or special columns for particularly preparative use with packing compression according to FIGS. 5 and 6.
  • the column is clamped in each case with constant force, which is predetermined by the clamping device and is therefore independent of the user.
  • a pressure element (6) is provided, which presses the clamping and sealing element (5) onto the column (2) via a punch (7), the necessary being provided by a lower bearing (4) and a lower clamping and sealing element (3) Back pressure is generated.
  • the stamp (7) can of course also be an integral part of the clamping and sealing element (5).
  • a pressure element (6) z. B. serve a spring element which is tensioned by lever pressure, e.g. in the manner of a toggle clamp. The required clamping force can also be applied with a pressure screw acting on the spring element.
  • a pneumatic cylinder is preferably used as the pressure element (6), which can be supplied by a compressed air line in the laboratory or an external compressed gas bottle.
  • the working stroke i.e. the distance covered by the upper tensioning and sealing element (5) when the column is clamped or relaxed should be at least about 10 to 20 mm, so that the column is freely accessible in the relaxed state and can be replaced without hindrance.
  • the lower bearing (4) should be adjustable in the tube. Either a continuous tube adjustment can be provided or different locking levels for columns in different standard lengths.
  • a new column is installed in such a way that, if necessary after adjusting the height of the lower bearing (4) to the column length, the column is inserted into the lower clamping and sealing element (3) and after aligning the column (2) with the help of a Centering piece (8) (eg in the form of a V-shaped receptacle), the pressure element (6) is actuated, as a result of which the upper tensioning and sealing element (5) is pressed onto the column (2).
  • Replacing a column therefore only takes a few seconds and can be carried out easily even by inexperienced personnel.
  • the constant contact pressure specified by the pneumatic cylinder or the spring force ensures that the column is securely sealed, but that the sealing elements are not overstressed.
  • the column change can also be completely automated with the device according to the invention.
  • An example of such a device is shown in FIG. 7, wherein several columns (2) are mounted on a rotating magazine (31).
  • the clamping device according to the invention has 2 pressure elements in the form of pneumatic cylinders (33) which move the clamping and sealing elements (32). By actuating the pneumatic cylinder, the column (2) is therefore released at both ends, and any other column can take its place by rotating the stand (31).
  • all types of columns can also be used here after appropriate adjustment of the clamping and sealing elements (32).
  • Other column changing devices can also be used instead of a rotating magazine.
  • the automatability made possible by the clamping device according to the invention allows, for example, separations of different substance samples which are present in sample tubes or on enrichment columns adsorbed in a column changing device according to FIG. 7 to be automatically pre-programmed on one or, if a changing device is used, for the separation column on different columns, e.g. to drain overnight.
  • the invention provides a valuable new device with which the field of application of liquid chromatographic separation processes can be expanded further.

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Treatment Of Liquids With Adsorbents In General (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Description

Die Erfindung betrifft eine Vorrichtung Zum Einspannen und schnellen Wechseln von Säulen für die Flüssigkeitschromatographie, wobei eine totvolumenfreie Verbindung von Säule und Anschlußstücken, die Zu-und Abführungen für das Laufmittel enthalten, durch Zusammenwirken von Dichtelementen der Säule und der Anschlußstücke erfolgt.The invention relates to a device for clamping and quickly changing columns for liquid chromatography, with a dead volume-free connection of the column and connecting pieces, which contain feeds and discharges for the eluent, by the interaction of sealing elements of the column and the connecting pieces.

Mit ausschlaggebend für qualitativ gute chromatographische Trennungen ist eine totvolumenfreie Verbindung zwischen de" - auswechselbaren - Trennsäule und den geräteseitig, d.h. stationär vorhandenen Zu- und Abführungen für das Laufmittel. Diese Verbindung sollte einerseits leicht lösbar sein, damit einfach und schnell ein Säulenwechsel stattfinden kann, sollte aber andererseits garantieren, daß auch nach oftmaligem Lösen und Zusammenfügen der Verbindung die Dichtigkeit und Totvolumenfreiheit gewahrt bleibt.Decisive for high-quality chromatographic separations is a dead volume-free connection between the " replaceable" separation column and the device-side, ie stationary inlets and outlets for the mobile phase. on the other hand, it should guarantee that even after the connection has been loosened and assembled frequently, the tightness and freedom from dead volume are maintained.

Bisher wurde diese Aufgabe so gelöst, daß die Kapillaren für die Laufmittelzu- und -abführung unter Verwendung von Schneid- bzw. Klemmringen aus Metall oder Kunststoff mit Druckschrauben an die eigentliche Säule angeschraubt wurden. Zur Reduzierung des Säulenguerschnitts auf den Querschnitt der Kapillarleitung sind die Säulen in der Regel beidseits mit Reduzierverschraubungen verschlossen, die auf die Säule geschraubt oder mit Schneidringverschraubungen aufgeklemmt werden.So far, this problem has been solved in such a way that the capillaries for the solvent supply and discharge were screwed onto the actual column using pressure or clamping rings made of metal or plastic with pressure screws. In order to reduce the column cross-section to the cross-section of the capillary line, the columns are usually closed on both sides with reducing screw connections, which are screwed onto the column or clamped on with cutting ring screw connections.

Eine Variante dieser Lösung besteht darin, daß die Säule als eine beidseits mit einem Filtermedium verschlossene Kartusche ausgeführt wird. Diese wird in ein Rohr mit beidseitigen Reduzierverschraubungen und Anschlußverschraubungen für die Kapillaren eingespannt. Vorteil dieser Konstruktion ist es, daß bei einem erforderlichen Säulenwechsel nur die das Sorbens enthaltende Kartusche ausgetauscht werden muß, wogegen die komplizierten und teuren Reduzierverschraubungen immer wieder benutzt werden können. Beim Kartuschenwechsel muß zumindest einseitig vor dem Abschrauben der Reduzierverschraubung zu, nächst die Kapillarleitung entfernt werden. Eine ähnliche Vorrichtung ist aus der US-A 3 682 315 bekannt.A variant of this solution is that the column is designed as a cartridge sealed on both sides with a filter medium. This is clamped into a tube with reducing fittings on both sides and connecting fittings for the capillaries. The advantage of this construction is that when the column has to be changed, only the cartridge containing the sorbent has to be replaced, whereas the complicated and expensive reducing screw connections can be used again and again. When changing the cartridge, the capillary line must be removed at least on one side before unscrewing the reducing screw. A similar device is known from US-A 3,682,315.

Alle diese Lösungen haben den Nachteil, daß die für eine gute Trennleistung der Säule wesentlichen Anschlußverbindungen durch manuelles Verschrauben hergestellt werden. Dabei besteht immer die Gefahr, daß entweder durch zu leichtes Anziehen keine vollständige Abdichtung erzielt wird oder durch zu festes Anziehen die Dichtelemente beschädigt werden. Ein schneller, sicherer Säulenwechsel auch durch nicht geübtes Personal ist damit nicht möglich. Auch ein automatisierter Säulenwechsel ist dabei kaum möglich.All these solutions have the disadvantage that the connection connections which are essential for a good separation performance of the column are produced by manual screwing. There is always the risk that either a too tight tightening will not achieve a complete seal or that the sealing elements will be damaged by overtightening. A quick, safe column change, even by inexperienced personnel, is therefore not possible. An automated column change is hardly possible.

Es bestand daher die Aufgabe, eine Einspannvorrichtung zu finden, die einen schnellen, gegebenenfalls auch automatisierbaren Säulenwechsel gestattet und die trotzdem eine verbesserte Sicherheit der Abdichtung gewährleistet.The object was therefore to find a clamping device which allows a quick, possibly also automated column change and which nevertheless ensures improved safety of the seal.

Diese Aufgabe wurde durch die vorliegende Erfindung gelöst.This object has been achieved by the present invention.

Gegenstand der Erfindung ist daher eine Vorrichtung zum Einspannen und schnellen Wechseln von Säulen für die Flüssigkeitschromatographie gemäß Anspruch 1.The invention therefore relates to a device for clamping and rapidly changing columns for liquid chromatography according to claim 1.

Das erfindungsgemäße Prinzip kann in unterschiedlicher Weise, abgestimmt auf spezielle Anforderungen, realisiert werden. In den Zeichnungen sind einige bevorzugte Ausgestaltungsmöglichkeiten dargestellt.

  • Figur 1 zeigt eine Aufsicht auf eine schematisiert dargestellte erfindungsgemäße Vorrichtung.
  • Figur 2 zeigt eine Seitenansicht der gleichen Vorrichtung.
  • Figur 3 zeigt einen Schnitt durch eine Ausführungsform eines Spann- und Dichtelementes in Verbindung mit einer Kartusche.
  • Figur 4 zeigt einen Schnitt durch eine Ausführungsform eines Spann- und Dichtelementes in Verbindung mit einer Säule mit Reduzierverschraubung.
  • Figur 5 zeigt einen Schnitt durch eine Ausführungsform eines Spann- und Dichtelementes in Verbindung mit einer Säule mit komprimierbarer Packung.
  • Figur 6 zeigt einen Schnitt durch eine Ausführungsform eines Spann- und Dichtelementes in Verbindung mit einer Säule mit komprimierbarer Packung und Membranabdichtung.
  • Figur 7 zeigt ein Beispiel einer automatisierbaren Anwendung der erfindungsgemäßen Einspannvorrichtung in Verbindung mit einer Säulenwechselvorrichtung.
The principle according to the invention can be implemented in different ways, tailored to special requirements. Some preferred design options are shown in the drawings.
  • Figure 1 shows a plan view of a schematically illustrated device according to the invention.
  • Figure 2 shows a side view of the same device.
  • Figure 3 shows a section through an embodiment of a clamping and sealing element in connection with a cartridge.
  • Figure 4 shows a section through an embodiment of a clamping and sealing element in connection with a column with reducing screw.
  • Figure 5 shows a section through an embodiment of a tensioning and sealing element in connection with a column with compressible packing.
  • Figure 6 shows a section through an embodiment of a tensioning and sealing element in connection with a column with compressible packing and membrane seal.
  • FIG. 7 shows an example of an automatable application of the clamping device according to the invention in connection with a column changing device.

In den Zeichnungen ist mit 1 eine Trägerplatte bezeichnet, mit 2 die Säule und mit 3 das untere Spann- und Dichtelement. 4 ist ein Lager, 5 das obere Spann- und Dichtelement und 6 ein Druckelement mit dem Stempel 7. Mit 8 ist ein Zentrierstück bezeichnet, g und 10 sind Kapillaren für die Laufmittelzu- und -abführung. 11 ist ein speziell für den Anschluß einer Kartusche gestalteter Dichtkegel, 12 die Säulenfüllung. 13 ist ein Dichtring mit eingepreßter Fritte 14, der mit einer aufgeklebten oder aufgepreßten Kappe 15 am Kartuschenende befestigt ist. Mit 16 ist eine Fritte und mit 17 ein Dichtring bezeichnet, die in eine Reduzierverschraubung 18 eingepreßt sind. 19 ist ein speziell auf Säulen mit Reduzierverschraubung angepaßtes Spann- und Dichtelement und 20 der entsprechende Dichtkonus. 21 ist eine Fritte, 22 eine Kugelschüttung und 23 eine Dichtung. 24 ist eine weitere ausführungsform eines Spann- und Dichtelementes. 25 ist eine flexible Membran und 26 eine Klemmkappe. Mit 27 ist ein Druckring zum festhalten der Klemmkappe 26 bezeichnet, mit 28 ein Stempel, mit 29 ein Spannelement und mit 30 ein Federelement. 31 ist ein Drehmagazin, 32 ein Spannund Dichtelement und 33 ein Pneumatikzylinder.In the drawings, 1 denotes a carrier plate, 2 the column and 3 the lower tensioning and sealing element. 4 is a bearing, 5 the upper tensioning and sealing element and 6 a pressure element with the stamp 7. A centering piece is designated by 8, g and 10 are capillaries for the solvent supply and discharge. 11 is a sealing cone specially designed for the connection of a cartridge, 12 is the column filling. 13 is a sealing ring with a pressed-in frit 14, which is fastened to the end of the cartridge with a glued-on or pressed-on cap 15. 16 with a frit and 17 denotes a sealing ring, which are pressed into a reducing screw 18. 19 is a clamping and sealing element specially adapted to columns with reducing screw connection and 20 the corresponding sealing cone. 21 is a frit, 22 a ball bed and 23 a seal. 24 is a further embodiment of a tensioning and sealing element. 25 is a flexible membrane and 26 is a clamping cap. With 27 a pressure ring for holding the clamping cap 26 is designated, with 28 a stamp, with 29 a clamping element and with 30 a spring element. 31 is a rotating magazine, 32 is a clamping and sealing element and 33 is a pneumatic cylinder.

Wie bereits aus den in den Zeichnungen dargestellten Beispielen ersichtlich ist, kann die erfindungsgemäße Vorrichtung in Verbindung mit allen möglichen Säulenkonstruktionen verwendet werden. Zur Anpassung an verschiedene Säulenkonstruktionen muß lediglich der Dichtteil des Spann- und Dichtelementes (5, 19/20, 24, 27/28) auf die Säule abgestimmt sein. Das erfindungsgemäße Prinzip, daß nämlich die Säule ohne Verschrauben zwischen 2 Spannund Dichtelemente eingespannt wird, bleibt davon unberührt. Es können daher sowohl die heute noch überwiegend gebräuchlichen Säulen mit Reduzierverschraubung entsprechend Figur 4 verwendet werden als auch Kartuschensäulen entsprechend Figur 3 oder auch Spezialsäulen für insbesondere präparative Anwendung mit Packungskompression entsprechend den Figuren 5 und 6.As can already be seen from the examples shown in the drawings, the device according to the invention can be used in connection with all possible column constructions. To adapt to different column designs, only the sealing part of the tensioning and sealing element (5, 19/20, 24, 27/28) must be matched to the column. The principle according to the invention, namely that the column is clamped between two clamping and sealing elements without screwing, remains unaffected. It can therefore both Columns according to FIG. 4 that are still predominantly used today are used as well as cartridge columns according to FIG. 3 or special columns for particularly preparative use with packing compression according to FIGS. 5 and 6.

Das Einspannen der Säule erfolgt jeweils mit konstanter, von der Einspannvorrichtung vorgegebener und daher vom Anwender unabhängiger Kraft. Dazu ist ein Druckelement (6) vorgesehen, das über einen Stempel (7) das Spannund Dichtelement (5) auf die Säule (2) drückt, wobei durch ein unteres Lager (4) und ein unteres Spann- und Dichtelement (3) der notwendige Gegendruck erzeugt wird. Der Stempel (7) kann selbstverständlich auch integraler Bestandteil des Spann- und Dichtelementes (5) sein. Als Druckelement (6) kann z. B. ein Federelement dienen, das durch Hebeldruck gespannt wird, z.B. in der Art eines Kniehebelspanners. Auch mit einer auf das Federelement wirkenden Druckschraube kann die erforderliche Spannkraft aufgebracht werden.The column is clamped in each case with constant force, which is predetermined by the clamping device and is therefore independent of the user. For this purpose, a pressure element (6) is provided, which presses the clamping and sealing element (5) onto the column (2) via a punch (7), the necessary being provided by a lower bearing (4) and a lower clamping and sealing element (3) Back pressure is generated. The stamp (7) can of course also be an integral part of the clamping and sealing element (5). As a pressure element (6) z. B. serve a spring element which is tensioned by lever pressure, e.g. in the manner of a toggle clamp. The required clamping force can also be applied with a pressure screw acting on the spring element.

Bevorzugt wird als Druckelement (6) jedoch ein Pneuma: tikzylinder verwendet, der durch eine im Labor vorhandene Druckluftleitung oder eine externe Druckgasflasche versorgt werden kann.However, a pneumatic cylinder is preferably used as the pressure element (6), which can be supplied by a compressed air line in the laboratory or an external compressed gas bottle.

Der Arbeitshub, d.h. der Weg, den das obere Spannund Dichtlement (5) beim Einspannen beziehungsweise Entspannen der Säule zurücklegt, sollte mindestens etwa 10 bis 20 mm betragen, so daß in entspanntem Zustand die Säule frei zugänglich ist und ohne Behinderung ausgetauscht werden kann. Zur Anpassung des Freiraumes zwischen dem oberen (5) und unteren Spann- und Dichtelement (3) an unterschiedliche Säulenlängen sollte das untere Lager (4) in der Röhe verstellbar sein. Dabei kann entweder eine kontinuierliche Röhenverstellung vorgesehen werden oder aber verschiedene Raststufen für Säulen in verschiedenen Standardlängen.The working stroke, i.e. the distance covered by the upper tensioning and sealing element (5) when the column is clamped or relaxed should be at least about 10 to 20 mm, so that the column is freely accessible in the relaxed state and can be replaced without hindrance. To adjust the free space between the upper (5) and lower clamping and sealing element (3) to different column lengths, the lower bearing (4) should be adjustable in the tube. Either a continuous tube adjustment can be provided or different locking levels for columns in different standard lengths.

Der Einbau einer neuen Säule erfolgt so, daß, gegebenenfalls nach Anpassung der Höhe des unteren Lagers (4) an die Säulenlänge, die Säule in das untere Spann- und Dichtelement (3) eingesetzt wird und nach Ausrichten der Säule (2) mit Hilfe eines Zentrierstücks (8) (z.B. in Form einer V-förmigen Aufnahme) das Druckelement (6) betätigt wird, wodurch das obere Spann- und Dichtelement (5) auf die Säule (2) aufgepreßt wird. Das Auswechseln einer Säule nimmt daher nur wenige Sekunden in Anspruch und kann auch von ungeübtem Personal problemlos ausgeführt werden. Durch den vom Pneumatikzylinder oder der Federkraft vorgegebenen konstanten Anpreßdruck ist dabei gewährleistet, daß die Säule zwar sicher abgedichtet ist, daß aber keine Überbeanspruchung der Dichtelemente erfolgt.A new column is installed in such a way that, if necessary after adjusting the height of the lower bearing (4) to the column length, the column is inserted into the lower clamping and sealing element (3) and after aligning the column (2) with the help of a Centering piece (8) (eg in the form of a V-shaped receptacle), the pressure element (6) is actuated, as a result of which the upper tensioning and sealing element (5) is pressed onto the column (2). Replacing a column therefore only takes a few seconds and can be carried out easily even by inexperienced personnel. The constant contact pressure specified by the pneumatic cylinder or the spring force ensures that the column is securely sealed, but that the sealing elements are not overstressed.

Der Säulenwechsel kann mit der erfindungsgemäßen Vorrichtung auch völlig automatisiert werden. Ein Beispiel einer solchen Einrichtung ist in Figur 7 gezeigt, wobei mehrere Säulen (2) auf ein Drehmagazin (31) montiert sind. Die erfindungsgemäße Einspannvorrichtung hat dabei 2 Druckelemente in Form von Pneumatikzylindern (33), die die Spann- und Dichtelemente (32) bewegen. Durch Betätigen der Pneumatikzylinder wird die Säule (2) daher an beiden Enden freigegeben und es kann durch Drehen des Ständers (31) jede beliebige andere Säule an deren Stelle treten. Selbstverständlich sind auch hier nach entsprechender Anpassung der Spann- und Dichtelemente (32) alle Arten von Säulen verwendbar. Ebenso können an Stelle eines Drehmagazins andere Säulenwechselvorrichtungen eingesetzt werden.The column change can also be completely automated with the device according to the invention. An example of such a device is shown in FIG. 7, wherein several columns (2) are mounted on a rotating magazine (31). The clamping device according to the invention has 2 pressure elements in the form of pneumatic cylinders (33) which move the clamping and sealing elements (32). By actuating the pneumatic cylinder, the column (2) is therefore released at both ends, and any other column can take its place by rotating the stand (31). Of course, all types of columns can also be used here after appropriate adjustment of the clamping and sealing elements (32). Other column changing devices can also be used instead of a rotating magazine.

Der Ausdruck 'Säule' ist in der vorliegenden Anmeldung in weitem Sinne zu verstehen. Es sind damit nicht nur die eigentlichen Trennsäulen gemeint, sondern auch Z.B. Vorsäulen, Anreicherungssäulen oder z.B. auch Proberöhrchen, die eine zu trennende Probe enthalten.The expression “column” is to be understood in a broad sense in the present application. This means not only the actual separation columns, but also e.g. Guard columns, enrichment columns or e.g. also test tubes that contain a sample to be separated.

Die durch die erfindungsgemäße Einspannvorrichtung ermöglichte Automatisierbarkeit erlaubt es Z.B., Trennungen von unterschiedlichen Substanzproben, die in Proberöhrchen oder auf Anreichungssäulen adsorbiert in einer Säulenwechselvorrichtung entsprechend Figur 7 vorliegen, an einer oder bei Einsatz einer Wechselvorrichtung auch für die Trennsäule an unterschiedlichen Säulen automatisch vorprogrammierbar, z.B. über Nacht ablaufen zu lassen. Durch die Erfindung steht eine wertvolle neue Vorrichtung zur Verfügung, mit der der Anwendungsbereich von flüssigkeitschromatographischen Trennverfahren weiter ausgebaut werden kann.The automatability made possible by the clamping device according to the invention allows, for example, separations of different substance samples which are present in sample tubes or on enrichment columns adsorbed in a column changing device according to FIG. 7 to be automatically pre-programmed on one or, if a changing device is used, for the separation column on different columns, e.g. to drain overnight. The invention provides a valuable new device with which the field of application of liquid chromatographic separation processes can be expanded further.

Claims (3)

1. Device for clamping and rapidly changing columns for liquid chromatography, whereby the column and connectors which are provided with inlets and outlets for the mobile phase are connected without dead volume due to the combined action of the sealing elements of the column and the connectors, characterised in that an upper (5) and a lower (3) clamping and sealing element, having sealing elements (11,20, 23 and 28) compatible with the design of the column are provided, at least one of these clamping and sealing elements (3,5) being movable along the axis of the column with the aid of a pressure element (6), it being possible for the column in the unclamped state to be moved in an axial direction and exchanged and, in the clamped state, the clamping and sealing elements (3,5), under a pre-set pressure, acting in combination with the column (2) to form a seal.
2. Device according to Claim 1, characterised in that the pressure element (6) is a pneumatic cylinder.
3. use of the evice according to Claim 1 in combination with a device for column changing (31).
EP82109585A 1981-10-30 1982-10-16 Clamping device for columns in chromatography Expired EP0078435B1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19813143075 DE3143075A1 (en) 1981-10-30 1981-10-30 COLUMN CLAMPING DEVICE FOR CHROMATOGRAPHY "
DE3143075 1981-10-30

Publications (3)

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EP0078435A2 EP0078435A2 (en) 1983-05-11
EP0078435A3 EP0078435A3 (en) 1983-06-22
EP0078435B1 true EP0078435B1 (en) 1986-02-05

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EP82109585A Expired EP0078435B1 (en) 1981-10-30 1982-10-16 Clamping device for columns in chromatography

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US (1) US4451365A (en)
EP (1) EP0078435B1 (en)
JP (1) JPS5883261A (en)
CA (1) CA1187816A (en)
CS (1) CS241127B2 (en)
DD (1) DD208553A5 (en)
DE (2) DE3143075A1 (en)
ES (1) ES516948A0 (en)

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Also Published As

Publication number Publication date
CA1187816A (en) 1985-05-28
CS241127B2 (en) 1986-03-13
ES8401258A1 (en) 1983-12-01
JPS5883261A (en) 1983-05-19
ES516948A0 (en) 1983-12-01
EP0078435A3 (en) 1983-06-22
DD208553A5 (en) 1984-04-04
US4451365A (en) 1984-05-29
DE3268996D1 (en) 1986-03-20
DE3143075A1 (en) 1983-05-11
CS769982A2 (en) 1985-07-16
EP0078435A2 (en) 1983-05-11

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